ホームMCPワークベンチSkills
ホームワークベンチ通知マイページ
llms.txt · MCPガイドプライバシーポリシー · 利用規約 · サポートv1.8.0
  1. ホーム
  2. /反応

Benzylamine → HCID 68514274、化合物

HRID 1717242
ノート
印刷プレビュー

反応式

HRID 1717242 の反応式
ClC(Cl)(O[C:5](=[O:11])OC(Cl)(Cl)Cl)Cl.[NH2:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]2[C:24]([CH2:25][CH2:26][CH3:27])=[C:23]([C:28]([NH:30][CH:31]3[CH2:33][CH2:32]3)=[O:29])[N:22]=[N:21]2)=[CH:16][CH:15]=1.C(N(CC)C(C)C)(C)C.[CH2:43]([NH2:50])[C:44]1[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=1>ClCCl.C(OCC)(=O)C>[CH2:43]([NH:50][C:5]([NH:13][C:14]1[CH:19]=[CH:18][C:17]([N:20]2[C:24]([CH2:25][CH2:26][CH3:27])=[C:23]([C:28]([NH:30][CH:31]3[CH2:32][CH2:33]3)=[O:29])[N:22]=[N:21]2)=[CH:16][CH:15]=1)=[O:11])[C:44]1[CH:49]=[CH:48][CH:47]=[CH:46][CH:45]=1
参加物実験手順後処理出典と根拠反応ノート

参加物

7

反応物 4

HCID 7504BenzylamineHCID 81531Diisopropylethylamine2 回HCID 94429TriphosgeneHCID 685175481-(4-aminophenyl)-N-cyclopropyl-5-propyl-1H-1,2,3-triazole-4-carboxamide

生成物 1

HCID 68514274HCID 68514274、化合物収率 52%

試薬・触媒・溶媒 2

HCID 6344
Dichloromethane
溶媒
3 回
HCID 8857Ethyl Acetate溶媒

実験手順

To a solution of triphosgene (0.08 g) in dichloromethane (7 ml) was added dropwise a solution of 1-(4-aminophenyl)-N-cyclopropyl-5-propyl-1H-1,2,3-triazole-4-carboxamide (0.21 g) obtained in Example 1d) and N,N-diisopropylethylamine (0.13 ml) in dichloromethane (3 ml) under ice-cooling, and the mixture was stirred under ice-cooling for 30 min. A solution of benzylamine (0.12 ml) and N,N-diisopropylethylamine (0.13 ml) in dichloromethane (3 ml) was added. The mixture was stirred at room temperature for 20 hr and diluted with ethyl acetate. The ethyl acetate solution was washed with water and saturated brine and dried over anhydrous magnesium sulfate. The solvent was evaporated under reduced pressure, and the residue was purified by silica gel column (hexane/ethyl acetate=1/1 to ethyl acetate). The resultant product was recrystallized from diethyl ether/methanol to give the title compound as a colorless powder (0.16 g, 52%).

後処理

  1. temperaturecooling
  2. temperaturecooling for 30 min
  3. stirringThe mixture was stirred at room temperature for 20 hr
  4. washThe ethyl acetate solution was washed with water and saturated brine
  5. dry with materialdried over anhydrous magnesium sulfate
  6. customThe solvent was evaporated under reduced pressure
  7. customthe residue was purified by silica gel column (hexane/ethyl acetate=1/1 to ethyl acetate)
  8. customThe resultant product was recrystallized from diethyl ether/methanol

出典と根拠

ORDレコード
ord-9318ead5d7964029a8b15862c4cfba3c
出典データセット
uspto-grants-2010_09
DOI
10.6084/m9.figshare.5104873.v1
特許番号
US07803822B2

反応ノート

読み込み中…

このページの内容参加物実験手順後処理出典と根拠反応ノート